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This presentation summarizes the latest results on the BAM-Themenfeld project SURDIA on processing of high-entropy alloys (HEAs) at BAM. At first, the influence of machining by ultrasonic-assisted milling on the surface integrity is presented. Second, the weld processing by Tungsten Inert Gas (TIG) welding is presented and the results of the Friction Stir Welding (FSW), which is conducted at BAM for the first time.
This study gives an overview on the important field of joining processes for component fabrication in hydrogen technologies. For that reason, the current need and future research and developement activites are highlighted for the different technological field of hydrogen generation, storage, transport and use. In addition, the emerging field of additive manufacturing is included. Finally, some remarks are given for necessary changes in the standardization and its challenges.
Martensitic 9 %-Cr steels like P91 and P92 show susceptibility to delayed hydrogen assisted cracking depending on their microstructure. In that connection, effective hydrogen diffusion coefficients are used to assess the possible time-delay. The small number of available diffusion coefficients varies already at room temperature by several orders of magnitude (mostly regarded as result of present microstructure). Especially P91 weld metal diffusion coefficients are rare so far. For that reason, electrochemical permeation experiments had been conducted using P92 base metal and P91 weld metal (in as-welded and heat-treated condition) with different thicknesses. The diffusion coefficients are calculated by two methods (time-lag and inflection point method) were performed. The results show that, despite of microstructural effects, the sample thickness must be considered as it influences the calculated diffusion coefficients. Finally, the comparison of calculated and measured hydrogen concentrations (determined by carrier gas hot extraction) enables the identification of realistic diffusion coefficients.
Hochentropie-Legierungen (HEAs) zeichnen sich durch einen Mischkristall-System aus mindestens fünf und Mittelentropie-Legierungen (MEAs) durch mindestens drei Hauptlegierungselemente aus, in äquiatomarer Zusammensetzung. Sie zeigen außergewöhnliche Anwendungseigenschaften, wie z.B. hohe Festigkeit, Duktilität oder Korrosionsbeständigkeit. Zukünftige HEA/MEA-Komponenten aufgrund ihrer Eigenschaften für wasserstoffhaltige Umgebungen (wie Behälter für kryogene oder Hochdruckspeicherung) von Interesse. Daher ist die Bewertung der Wasserstoffabsorption und die Diffusion in diesen Materialien von großer Bedeutung. Dazu wurden in unserer Studie eine CoCrFeMnNi-HEA und eine CoCrNi-MEA untersucht. Die Proben wurden elektrochemisch mit Wasserstoff beladen. Für die Ermittlung des Wasserstoffdiffusionsverhaltens wurde die thermische Desorptionsanalyse (TDA) mit unterschiedlichen Heizraten bis zu 0,250 K/s angewandt. Die nachfolgende Peakentfaltung der Signale führte zu Hochtemperatur-Desorptionsspitzen und Wasserstofftrapping auch über 280°C. Eine resultierende Gesamtwasserstoffkonzentration > 40 ppm wurde für den MEA ermittelt und > 100 ppm für den HEA. Dies deutet auf zwei wichtige Effekte hin:
(1) verzögerte Wasserstoffdiffusion und (2) eine beträchtliche Menge an getrapptem Wasserstoff auch bei hoher Temperatur. Beide Effekte können hinsichtlich einer wasserstoffunterstützten Rissbildung kritisch werden, dies erfordert jedoch weitere Untersuchungen. Zusätzlich erfolgte die Bestimmung des lokalen Volta-Potentials mittels hochauflösender Kelvin-Sonden-Kraft-Mikroskopie (SKPFM). Die ermittelten Scans zeigen einen bestimmten Einfluss der Wasserstoffbeladung auf die Potentiale.
HEAs represent a relatively new class of materials. The the alloy concept is fundamentally different from the most conventional materials and alloys that are used today. Recently, the focus of HEA designs is more application-based. For that purpose, the elements of interest are carefully selected and multiple phases as well as micro-structures are deliberately adjusted. Currently, only limited attention has been paid to weldability of HEA. This encompasses possible effects on metallurgy and its influence on the desired properties. It remains open if welding causes e.g. considerable number of intermetallic phases or segregations and their effect on weld joint properties. For that reason, the scope of this study is to summarize already available studies on welding of HEAs with respect to the HEA-type, the applied welding process and its influence on the weld joint properties.
9 %-Cr steel P91 is widely used in power plants due to the excellent creep-resistance. Components of this steel are typically welded and demand for careful welding fabrication, whereas a so-called post weld heat treatment (PWHT), must be conducted to increase the toughness and decrease the hardness of the martensitic as-welded (AW) microstructure. Before the PWHT, a hydrogen removal (or dehydrogenation) heat treatment is necessary as hardened AW martensitic microstructure is generally prone to delayed hydrogen assisted cracking (HAC). The microstructure and temperature dependent hydrogen diffusion is an important issue as it determines how long a potential crack-critical hydrogen concentration could remain in the microstructure. In this context, reliable hydrogen diffusion coefficients of P91 weld metal are rare. Hence, the diffusion behavior of P91 multi-layer weld metal was investigated in two different microstructure conditions: AW and further PWHT (760 °C for 4 h). Two different experimental techniques were used to cover a wide range of hydrogen diffusion temperatures: the electrochemical permeation technique (PT) at room temperature and the carrier gas hot extraction (CGHE) for a temperature range from 100 to 400 °C. From both techniques typical hydrogen diffusion coefficients were calculated and the corresponding hydrogen concentration was measured. It was ascertained that both heat treatment conditions show significant differences in hydrogen diffusivity. The biggest deviations were identified for room temperature. In this case, the AW condition shows significant hydrogen trapping and up to seven times lower diffusion coefficients. Additionally, PT investigations showed a preferred diffusion direction of hydrogen in the weld metal expressed by the diffusion coefficients and the permeability for both heat treatment conditions. The CGHE generally revealed lower diffusion coefficients for the AW microstructure up to 200 °C. In addition, the AW condition showed hydrogen concentrations up to 50 ml/100 g (considering electrochemical charging). Nonetheless, this hydrogen was not permanently (reversibly) trapped. Nonetheless, this temperature is approximately 100 °C below recommended dehydrogenation heat treatment (DHT). This has two main consequences: (I) in case of welding is interrupted or no DHT is conducted, a HAC susceptibility of hardened martensitic P91 weld metal cannot be excluded and (II) DHT can be conducted at temperatures around 200 °C below the recommended temperatures.
Hydrogen was once called “the versatile embrittler” [1], which summarizes very well the effect on reduction of ductility and/or toughness in technical alloys like steel. In that connection, welding is one of the most important component fabrication technologies. During welding, hydrogen can be transferred to the weld pool from manifold sources (like contaminations, residuals at the surface, etc.). As hydrogen embrittles a material, the safety of welded components with hydrogen is always a critical issue. Weld heat input causes additional changes in the microstructure like grain growth or partial dissolution of precipitates and many more. All these things influence the mechanical properties and also represent hydrogen traps. These traps decrease the hydrogen diffusion compared to the ideal lattice. The result can be so-called delayed hydrogen assisted cracking (HAC) of the weld joint due to the significantly decreased diffusivity by trapped hydrogen. This is often an underestimated risk as those cracks can appear in the weld joint even after some days!
It is essential to know about hydrogen ingress during welding and the microstructure specific hydrogen diffusion. Both are depended on weld parameter influence and the chemical composition of the base material and weld metal. For that purpose, gas analytic methods like solid-state carrier gas hot extraction (CGHE) are useful tools to: (1) identify detrimental hydrogen concentrations from weld joints, (2) binding energies from hydrogen traps by thermal desorption analysis or (3) high-temperature diffusion coefficients. Those values are extremely important for welding practice in terms of recommendations on realistic hydrogen removal heat treatment (HRHT) after welding. Considering the increasing use of “digital” experiments, the data is also needed for reliable numerical simulations of HAC process or HRHT-effectiveness.
The present contribution gives an overview on the influence of hydrogen on weld joints, the necessity, methods and standards for hydrogen determination (CGHE) with the aim of fabrication of safe welded and crack-free components.
[1] R. A. Oriani (1987), Corrosion 43(7):390-397. doi: 10.5006/1.3583875
High-strength low-alloyed (HSLA) steels with yield strength ≥ 690 MPa are gaining popularity in civil engineering and construction of heavy vehicles. With increasing yield strength, the susceptibility for degradation of the mechanical properties in presence of diffusible hydrogen, i.e. hydrogen-assisted cracking (HAC) generally increases. HAC is a result of the critical interaction of local microstructure, mechanical load and hydrogen concentration. In existing standards for welding of HSLA steels, recommendations (preheating, interpass temperature and hydrogen removal heat treatment) are given to limit the amount of introduced hydrogen during welding. The recommendations are based on investigations with conventional arc welding processes. In the past decade, modern weld technologies were developed to enable welding of narrower weld seams with V-grooves of 30°, e.g. the modified spray arc process. In that connection, a reduced number of weld runs and weld volume are important technical and, hence, economic benefits. In the present study, the hydrogen distribution in S960QL multi-layer welds with thickness of 20 mm was analyzed depending on heat control. The influence of different weld seam opening angles (grooves), heat input, interpass temperature and hydrogen removal procedures was investigated. The results show that weldments with narrow groove contained increased diffusible hydrogen amount. Reasons had been longer diffusion path and higher wire feeding rate compared to conventional welds with wider 60° Vgroove. Hydrogen concentration has been reduced by decreasing both the heat input and interpass temperature. Hydrogen free weldments were achieved via hydrogen removal heat treating at 250 °C for 5 h subsequently after welding. Regarding the strength of the investigated steel, it is recommended to conduct a heat treatment after welding. For the first time, hydrogen concentration gradients were experimentally determined across the weld seam thickness in HSLA multi-layer welds.
Hydrogen determination in weld seams is standardized in ISO 3690. In accordance to this standard, a defined time for hydrogen collection has to be anticipated for different extraction temperatures. In other words, the temperature is the most important value that has to be monitored in addition to the aimed hydrogen determination.
The specimen geometry has influence on the real sample temperature during CGHE vs. the adjusted furnace temperature. This presentation gives a short summary on possible influences on the "correct" hydrogen determination temperature during carrier gas hot extraction (CGHE) using infrared radiation driven furnace. The main findings are: (1) specimen surface is important in terms of polished or oxidized condition, (2) specimen geometry is important for fast heating, (3) PID-values of control software are a considerable influence to accelerate the heating process depite thick specimens and (4) independent sample temperature determination before CGHE is strongly recommended.